CN101774561A - Preparation process of large-particle food-grade calcium hydrophosphate - Google Patents
Preparation process of large-particle food-grade calcium hydrophosphate Download PDFInfo
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- CN101774561A CN101774561A CN201010102842A CN201010102842A CN101774561A CN 101774561 A CN101774561 A CN 101774561A CN 201010102842 A CN201010102842 A CN 201010102842A CN 201010102842 A CN201010102842 A CN 201010102842A CN 101774561 A CN101774561 A CN 101774561A
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- Prior art keywords
- reaction
- crystallizer
- draft tube
- lime carbonate
- food
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002245 particle Substances 0.000 title claims abstract description 21
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title abstract description 5
- 239000011575 calcium Substances 0.000 title abstract description 5
- 229910052791 calcium Inorganic materials 0.000 title abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 59
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 15
- 239000012452 mother liquor Substances 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 8
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 claims description 37
- 235000013305 food Nutrition 0.000 claims description 31
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 30
- 238000005516 engineering process Methods 0.000 claims description 23
- 235000019700 dicalcium phosphate Nutrition 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011344 liquid material Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 2
- 238000005119 centrifugation Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 229940088598 enzyme Drugs 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
A preparation process of large-particle food-grade calcium hydrophosphate is characterized by comprising the following steps: adding the calcium carbonate suspension and phosphoric acid into a DTB crystallizer in a continuous feeding mode to react, wherein the molar ratio of calcium carbonate to phosphoric acid is 1: 1; stirring speed of the DTB crystallizer is 800-1000 r/min during reaction, and reaction mother liquor which overflows from the DTB crystallizer and carries particles is circularly added into the crystallizer during reaction; the pH value of the reaction material in the DTB crystallizer is 5-6; the average residence time of the reaction materials in the DTB crystallizer is 40-50 minutes; centrifugal drying: and large-particle calcium hydrophosphate generated by the reaction is continuously discharged from the bottom through a settling zone at the lower part of the DTB crystallizer, and a finished product is obtained through centrifugation and drying. The invention has simple process flow and convenient operation, and the produced calcium hydrophosphate has large particles and good quality and is easy to filter and dry.
Description
Technical field
The present invention relates to a kind of preparation method's of secondary calcium phosphate, particularly a kind of large grained food-grade calcium hydrogen phosphate preparation technology.
Background technology
Phosphoric acid salt extensively is used in various flour products at home and abroad as foodstuff additive, milk preparation, the freezing grade in the food.Phosphorus and calcium are two kinds of important elements in the organism, can promote the metabolism of organism, are the important composition elements of bone, hormone, enzyme, VITAMIN etc.Double decomposition and direct two kinds of technologies of neutralisation are mainly adopted in the preparation of the secondary calcium phosphate of food grade at present.But the calcium hydrogen phosphate particle that ordinary process is produced is too thin, brings difficulty for subsequent handlings such as dehydration, drying.The flowability of product is poor simultaneously, has flown upward dirt in the use easily, loses bigger.At present, the preparation research to oarse-grained secondary calcium phosphate has some reports both at home and abroad, but mostly is to adopt the mode of adding some particle promotor to impel crystal structure and growth.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, provides that a kind of technical process calcium hydrogen phosphate particle simple, easy to operate, that produced is big, the preparation technology of the measured large grained food-grade calcium hydrogen phosphate of matter.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of preparation technology of large grained food-grade calcium hydrogen phosphate, is characterized in, its step is as follows:
(1) reaction: water is formulated as the lime carbonate suspension liquid that mass concentration is 20-30% with raw material food grade lime carbonate, adopt the successive feed way to join draft tube baffle crystallizer lime carbonate suspension liquid and raw material food grade phosphoric acid and react, the food grade lime carbonate that is added and the mol ratio of food grade phosphoric acid are 1: 1; The mixing speed of draft tube baffle crystallizer is 800～1000r/min during reaction, and the reaction mother liquor circulation of the entrained particles that in the time of reaction the draft tube baffle crystallizer top is overflowed joins in the crystallizer; The pH value of the reaction mass in the draft tube baffle crystallizer is 5-6; The mass ratio of the add-on of circulating mother liquor and food grade lime carbonate is 4-6: 1; The mean residence time of reaction mass in draft tube baffle crystallizer is 40-50 minute;
(2) centrifugal drying: the macrobead secondary calcium phosphate that reaction generates is discharged from the bottom continuously through the negative area of draft tube baffle crystallizer bottom, through centrifugal, the dry finished product that gets.
Technical problem to be solved by this invention can also further realize by following technical scheme.The preparation technology of above-described large grained food-grade calcium hydrogen phosphate is characterized in, in step (1): the mass ratio of the add-on of circulating mother liquor and food grade lime carbonate is 5: 1.
Technical problem to be solved by this invention can also further realize by following technical scheme.The preparation technology of above-described large grained food-grade calcium hydrogen phosphate is characterized in, in step (1): the pH value of the reaction mass in the draft tube baffle crystallizer is 5.5.
Technical problem to be solved by this invention can also further realize by following technical scheme.The preparation technology of above-described large grained food-grade calcium hydrogen phosphate is characterized in, in step (2): centrifugal gained filtrate replenishing is used for the preparation of lime carbonate suspension liquid.
Technology utilization food grade phosphoric acid of the present invention (its concentration can be the delicatessen food level concentration of phosphoric acid of routine) and calcium carbonate reaction generate secondary calcium phosphate, according to the kinetics of crystallization principle, introduce draft tube baffle crystallizer, and processing condition such as the degree of supersaturation by secondary calcium phosphate in the control reactive system, stirring intensity make the high-purity secondary calcium phosphate of macrobead.
Phosphoric acid and calcium carbonate reaction generate secondary calcium phosphate.This reaction is the acid-base neutralisation reaction, and speed of response is very fast, and secondary calcium phosphate is slightly soluble in water, and a large amount of secondary calcium phosphate crystal that generates has little time to grow up and just separates from reaction system fast, makes that the particulate granularity that generates is superfine.Synthetic reaction nucleation and two dynamic processes that take place, finish simultaneously simultaneously of particle crystal growth of comprising in the technology of the present invention.Because crystal growth is slower usually, the factor that is beneficial to the reaction nucleation is unfavorable for that generally particle grows up, thereby the design of reaction conditions is mainly from control crystal grain quantity be beneficial to the angle that particle grows up and consider.Technology of the present invention is introduced draft tube baffle crystallizer according to the kinetics of crystallization principle, reduces the speed of reaction in reaction process by the degree of supersaturation of secondary calcium phosphate in the control reaction system.Promptly in the process of crystallizer continuous charging, add reaction mother liquor, control the degree of supersaturation of reaction system by circulation.In reaction process, rationally control reaction mass simultaneously in the residence time of crystallizer, the processing condition such as mixing speed of crystallizer.Draft tube baffle crystallizer inside is provided with shutter, and crystalline growth district and crystallization negative area are separated, and does not disturb mutually, makes uniform crystal particles, stable, and the size of crystallization control particle size within the specific limits.The macrobead secondary calcium phosphate that generates is discharged continuously from the crystallizer bottom.
Compared with prior art, the major advantage of technology of the present invention is embodied in the following aspects:
1) explained hereafter of the present invention secondary calcium phosphate not only particle is big, quality is good, and filters easily and dry.The secondary calcium phosphate particle diameter that this explained hereafter goes out is greatly improved than general technology.The particle diameter of the secondary calcium phosphate that general technology is produced is below 20 μ m, and the product cut size that this explained hereafter goes out can reach 70 μ m.
2), the preparation of macrobead secondary calcium phosphate need consider that reducing crystal grain generates and strengthen two aspects of grain growing, is main and strengthen grain growing.Have a certain amount of crystal seed in the reaction system and exist, help the growth of nucleus.
3), technical process of the present invention is simple, easy to operate, can continuous production, also can batch production.
Embodiment
Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.
Embodiment 1.A kind of preparation technology of large grained food-grade calcium hydrogen phosphate, its step is as follows:
(1) reaction: it is 30% lime carbonate suspension liquid that water is formulated as mass concentration with raw material food grade lime carbonate, adopt the successive feed way to join draft tube baffle crystallizer lime carbonate suspension liquid and raw material food grade phosphoric acid and react, the food grade lime carbonate that is added and the mol ratio of food grade phosphoric acid are 1: 1; The mixing speed of draft tube baffle crystallizer is 1000r/min during reaction, and the reaction mother liquor circulation of the entrained particles that in the time of reaction the draft tube baffle crystallizer top is overflowed joins in the crystallizer; The pH value of the reaction mass in the draft tube baffle crystallizer is 6; The mass ratio of the add-on of circulating mother liquor and food grade lime carbonate is 6: 1; The mean residence time of reaction mass in draft tube baffle crystallizer is 50 minutes;
(2) centrifugal drying: the macrobead secondary calcium phosphate that reaction generates is discharged from the bottom continuously through the negative area of draft tube baffle crystallizer bottom, through centrifugal, the dry finished product that gets.
Embodiment 2.A kind of preparation technology of large grained food-grade calcium hydrogen phosphate, its step is as follows:
(1) reaction: it is 20% lime carbonate suspension liquid that water is formulated as mass concentration with raw material food grade lime carbonate, adopt the successive feed way to join draft tube baffle crystallizer lime carbonate suspension liquid and raw material food grade phosphoric acid and react, the food grade lime carbonate that is added and the mol ratio of food grade phosphoric acid are 1: 1; The mixing speed of draft tube baffle crystallizer is 800r/min during reaction, and the reaction mother liquor circulation of the entrained particles that in the time of reaction the draft tube baffle crystallizer top is overflowed joins in the crystallizer; The pH value of the reaction mass in the draft tube baffle crystallizer is 5; The mass ratio of the add-on of circulating mother liquor and food grade lime carbonate is 4: 1; The mean residence time of reaction mass in draft tube baffle crystallizer is 40 minutes;
(2) centrifugal drying: the macrobead secondary calcium phosphate that reaction generates is discharged from the bottom continuously through the negative area of draft tube baffle crystallizer bottom, through centrifugal, the dry finished product that gets.
Embodiment 3.A kind of preparation technology of large grained food-grade calcium hydrogen phosphate, its step is as follows:
(1) reaction: it is 25% lime carbonate suspension liquid that water is formulated as mass concentration with raw material food grade lime carbonate, adopt the successive feed way to join draft tube baffle crystallizer lime carbonate suspension liquid and raw material food grade phosphoric acid and react, the food grade lime carbonate that is added and the mol ratio of food grade phosphoric acid are 1: 1; The mixing speed of draft tube baffle crystallizer is 900r/min during reaction, and the reaction mother liquor circulation of the entrained particles that in the time of reaction the draft tube baffle crystallizer top is overflowed joins in the crystallizer; The pH value of the reaction mass in the draft tube baffle crystallizer is 5.5; The mass ratio of the add-on of circulating mother liquor and food grade lime carbonate is 5: 1; The mean residence time of reaction mass in draft tube baffle crystallizer is 45 minutes;
(2) centrifugal drying: the macrobead secondary calcium phosphate that reaction generates is discharged from the bottom continuously through the negative area of draft tube baffle crystallizer bottom, through centrifugal, the dry finished product that gets.
Embodiment 4.In the preparation technology's of embodiment 1 or 2 or 3 described large grained food-grade calcium hydrogen phosphates the step (2): centrifugal gained filtrate replenishing is used for the preparation of lime carbonate suspension liquid.
Claims (4)
1. the preparation technology of a large grained food-grade calcium hydrogen phosphate is characterized in that, its step is as follows:
(1) reaction: water is formulated as the lime carbonate suspension liquid that mass concentration is 20-30% with raw material food grade lime carbonate, adopt the successive feed way to join draft tube baffle crystallizer lime carbonate suspension liquid and raw material food grade phosphoric acid and react, the food grade lime carbonate that is added and the mol ratio of food grade phosphoric acid are 1: 1; The mixing speed of draft tube baffle crystallizer is 800～1000r/min during reaction, and the reaction mother liquor circulation of the entrained particles that in the time of reaction the draft tube baffle crystallizer top is overflowed joins in the crystallizer; The pH value of the reaction mass in the draft tube baffle crystallizer is 5-6; The mass ratio of the add-on of circulating mother liquor and food grade lime carbonate is 4-6: 1; The mean residence time of reaction mass in draft tube baffle crystallizer is 40-50 minute;
(2) centrifugal drying: the macrobead secondary calcium phosphate that reaction generates is discharged from the bottom continuously through the negative area of draft tube baffle crystallizer bottom, through centrifugal, the dry finished product that gets.
2. the preparation technology of large grained food-grade calcium hydrogen phosphate according to claim 1 is characterized in that, in step (1): the mass ratio of the add-on of circulating mother liquor and food grade lime carbonate is 5: 1.
3. the preparation technology of large grained food-grade calcium hydrogen phosphate according to claim 1 is characterized in that, in step (1): the pH value of the reaction mass in the draft tube baffle crystallizer is 5.5.
4. according to the preparation technology of claim 1 or 2 or 3 described large grained food-grade calcium hydrogen phosphates, it is characterized in that in step (2): centrifugal gained filtrate replenishing is used for the preparation of lime carbonate suspension liquid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010102842A CN101774561A (en) | 2010-01-29 | 2010-01-29 | Preparation process of large-particle food-grade calcium hydrophosphate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010102842A CN101774561A (en) | 2010-01-29 | 2010-01-29 | Preparation process of large-particle food-grade calcium hydrophosphate |
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| CN101774561A true CN101774561A (en) | 2010-07-14 |
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| CN201010102842A Pending CN101774561A (en) | 2010-01-29 | 2010-01-29 | Preparation process of large-particle food-grade calcium hydrophosphate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058249A (en) * | 2013-01-05 | 2013-04-24 | 刘立文 | Equipment and process for producing food-grade calcium carbonate by gypsum |
| CN103787295A (en) * | 2014-02-27 | 2014-05-14 | 南京工业大学 | Preparation technology of large-granular food-grade calcium hydrophosphate |
| CN106829904A (en) * | 2017-02-28 | 2017-06-13 | 连云港市德邦精细化工有限公司 | A kind of preparation method of graininess calcium phosphate dibasic anhydrous |
| CN106892413A (en) * | 2015-12-17 | 2017-06-27 | 中国科学院大连化学物理研究所 | The method that direct crystallization prepares ammonium dihydrogen phosphate in microreactor |
| CN117923447A (en) * | 2024-03-20 | 2024-04-26 | 云南磷化集团有限公司 | Method and device for continuously producing calcium hydrophosphate by cascade reaction kettles |
-
2010
- 2010-01-29 CN CN201010102842A patent/CN101774561A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058249A (en) * | 2013-01-05 | 2013-04-24 | 刘立文 | Equipment and process for producing food-grade calcium carbonate by gypsum |
| CN103787295A (en) * | 2014-02-27 | 2014-05-14 | 南京工业大学 | Preparation technology of large-granular food-grade calcium hydrophosphate |
| CN106892413A (en) * | 2015-12-17 | 2017-06-27 | 中国科学院大连化学物理研究所 | The method that direct crystallization prepares ammonium dihydrogen phosphate in microreactor |
| CN106892413B (en) * | 2015-12-17 | 2018-12-14 | 中国科学院大连化学物理研究所 | The method that direct crystallization prepares ammonium dihydrogen phosphate in microreactor |
| CN106829904A (en) * | 2017-02-28 | 2017-06-13 | 连云港市德邦精细化工有限公司 | A kind of preparation method of graininess calcium phosphate dibasic anhydrous |
| CN106829904B (en) * | 2017-02-28 | 2019-02-12 | 连云港市德邦精细化工有限公司 | A kind of preparation method of graininess calcium phosphate dibasic anhydrous |
| CN117923447A (en) * | 2024-03-20 | 2024-04-26 | 云南磷化集团有限公司 | Method and device for continuously producing calcium hydrophosphate by cascade reaction kettles |
| CN117923447B (en) * | 2024-03-20 | 2024-06-04 | 云南磷化集团有限公司 | Method and device for continuously producing calcium hydrophosphate by cascade reaction kettles |
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Open date: 20100714 |